Black sulfur dye.



UNITED STATES PATENT OFFICE.

PAUL JULllTS, OF LUDlVIGSHAFEN, GERMANY, ASSIGNDR TO THE BADIS CHE 'ANILIN AND SODA FABRIK, OF SAME PLACE.

BLACK SULFUR DYE.

SPECIFICATION forming part of Letters l atent No. 648,7 55, dated May 1, 1900.

Application filed February 6, 1900.

To It whom it may con-earn: Be it known that I, PAUL JULIUS, doctor of philosophy, a subject of the Emperor of Austria-Hungary, residing at Ludwigshafen-onthe-Rhine, in the Kingdom of Bavaria and Empire of Germany, have invented new and useful Improvements in Black Dyestuffs, of which the following is a specification.

My invention relates to the manufacture of a new deep-black'dyestuff which dyes cotton without the aid of a mordant. This dyestufi is obtained by treating a certain meta-phenylendiamin derivative with sulfur and sodium sulfid. The said meta-phenylendiamin derivative results from the condensation in alcoholic solution of a molecule of symmetrical dinitro-meta-di-ehlorbenzcne and two molecules of para-amidophenol in the presence of a body that will bind hydrochloric acid, such as sodium carbonate or acetate. In this way dinitro-di-para-liydroxy-diphenyl-metaphenylencdiamin is obtained which, judging from its manner of formation, has the following constitutional formula:

apparatus a mixture of one (1) molecular proportion of dinitro-di-chlorbenzenewith two (2) molecular proportions of para amido- Serial No. 4,264 I (No specimens.)

phenol hydrochlorid dissolved in alcohol and sufficient sodium acetate to bind the hydrochloric acid formed during the reaction. Continue the'heating until the dinitro-di-chlorbenzene has practically disappeared. Allow the liquid to cool andisolate the reaction productin any well-known manner. Mix together twenty (20) parts of the 'dinitro-dipara h ydroxy diphenyl meta phenylendiamin thus obtained with forty (40) parts of.

sulfur, one hundred and twenty (120) parts of crystallized sodium sulfid, and five (5) parts of water in' an iron vessel. Gradually heat the mixture to about. 140 centigrade while stirring and maintain at this temperature until the melt has become quite dry. Powder up the melt when cool. In this condition it can be directly used for dyeing purposes, or it may be dissolved in a little water 7 and the coloring-matter-salted outwith common salt. Inthis case it is necessary in addition to soda and common salt to add sodium sulfid to thedyeiug-bath in order to? obtain the best results. a

My new coloring-matter is readily soluble in water, its aqueous solution being deep blue. Acids added to this solution produce av brown precipitate which is redissolved by alkalies with a blue color. It dyesuninor danted cotton a deep black which is exceedingly fast to soap, light, and acids. It isbut little altered in fastness or shade, by subse quent treatment with chromates, copper salts, and the like.

Now what I claim is I A The new coloring-1natter which can be ob,-v

tained from dinitro l di para -l1ydroxy diphenyl-meta-phenylendiamin sulfur and so;- dium sulfid, whose solution in water is of a deep-blue color, dyeing unmordanted cotton a deep black, which is not materially altered in shade or fastn'ess by treatment with chromates and copper salts, and in which solution a brown precipitate is formed on the addition of hydrochloric acid, said precipitate dissolving in alkalies with a deep-blue color substantially as described.

In testimony whereof I have hereunto set my hand in the presence of two subscribing witnesses.

PAUL JULIUS. Witnesses:

JACOB ADRIAN, ERNEST F. EHRHARDT. 

